CN110265644A - A kind of preparation method of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery - Google Patents

A kind of preparation method of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery Download PDF

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CN110265644A
CN110265644A CN201910548720.4A CN201910548720A CN110265644A CN 110265644 A CN110265644 A CN 110265644A CN 201910548720 A CN201910548720 A CN 201910548720A CN 110265644 A CN110265644 A CN 110265644A
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carbon cloth
polyacrylic acid
porous structures
antimony pentoxide
reticulated porous
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CN110265644B (en
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费杰
王娜
黄剑锋
曹丽云
许占位
李嘉胤
郑欣慧
李盟
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Shaanxi University of Science and Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • H01M4/622—Binders being polymers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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Abstract

The present invention relates to a kind of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery preparation methods, step 1: carbon cloth is placed in acetone cleaning, drying after immersion, and the carbon cloth leaching of drying is placed in coating processing in polyacrylic acid aqueous solution and cleaning is dried again；Step 2: antimony trichloride is added to formation antimony trichloride solution in dehydrated alcohol, and addition sodium hydrate aqueous solution adjusts its pH and obtains mixed liquor in antimony trichloride solution；It is impregnated in carbon cloth merging mixed liquor after coating processing；Step 3: step 2 gained carbon cloth and mixed liquor go to hydro-thermal reaction in reaction kettle, are cooled to room temperature, and cleaning, drying obtains antimony pentoxide/polyacrylic acid/carbon cloth flexibility anode material of lithium-ion battery of reticulated porous structures.Its is easy to operate, reproducible, which combines the height ratio capacity feature of carbon cloth satisfactory mechanical property and antimony pentoxide, improves the electrochemistry cycle performance as anode material of lithium-ion battery.

Description

A kind of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility sodium ion The preparation method of cell negative electrode material
Technical field
The invention belongs to flexible energy storage material technical fields, and in particular to and a kind of antimony pentoxide of reticulated porous structures/ Polyacrylic acid/carbon cloth flexibility anode material of lithium-ion battery preparation method.
Background technique
With the development of flexible, flexible electronic device, developing, there is the flexible electrode material of height ratio capacity to have become mesh The important directions of preceding energy storage field research.Current main flexible electrode material generallys use the carbon material of good conductivity, such as stone Black alkene, carbon nanotube, carbon cloth etc..Wherein carbon cloth is used as flexibility because of its good mechanical strength, electric conductivity and flexibility extensively Electrode material substrate.In recent years, many researchers are used for flexible electrical by growing metal oxide isoreactivity substance on carbon cloth Pole material.NiO nanometer sheet is grown directly upon in carbon cloth substrate by LongH etc. by solwution method and annealing method, and is used as Lithium ion battery flexibility cathode (Growth of hierarchal mesoporous NiO nanosheets on carbon cloth as binder-free anodes for high-performance flexible lithium-ion batteries[J].ScientificReports,2014,4:7413).ZhangY etc. is prepared for a kind of soft by solvent-thermal method The MoSe of property2/ CF composite material (MoSe2 nanosheets grown on carbon cloth with superior electrochemical performance as flexible electrode for sodium ion batteries [J].RSC Advances,2015,6(2):1440-1444).SangHJ etc. synthesizes Na by sol-gal process2FeP2O7With it is more Hole carbon cloth composite material has good long-term circulation ability (Approach to as sodium-ion battery flexibility negative electrode material flexible Na-ion batteries with exceptional rate capability and long lifespan using Na2FeP2O7 nanoparticles on porous carbon cloth[J].Journal of Materials Chemistry A,2017,5(11):5502-5510).RenWN etc. passes through atomic layer deposition TiO2Layer is three-dimensional flower-shaped to modify MoS2Nanometer sheet carbon cloth composite material (ALD TiO2 coated flower-like MoS2 nanosheets on carbon cloth as sodium ion battery anode with enhanced cycling stability andrate capability[J].ACS Applied Materials&Interfaces,2016,9(1):487-495).However, above-mentioned side Carbon cloth is not involved in method to be combined therebetween with the active material of load and growth morphology homogeneity question.
Sodium ion battery negative research is concentrated mainly on carbon material, alloy material and chemical combination class material.Often Kind material has superiority and inferiority, and wherein metal compound material is widely studied since specific capacity is big.China is antimony product specie big country, antimony Positioned at the 5th main group of the periodic table of elements, there are two kinds of valence states of trivalent and pentavalent, corresponding oxide is Sb2O3And Sb2O5.Wherein, Sb2O3Theoretical capacity (1102mAhg with higher-1), and by numerous studies, and Sb2O5The report for making battery material does not go out temporarily It is existing.
Summary of the invention
The object of the present invention is to provide a kind of good netted more of easy to operate, at low cost, environmentally protective and binding force Antimony pentoxide/polyacrylic acid of pore structure/carbon cloth flexibility anode material of lithium-ion battery preparation method, antimony pentoxide It grows into reticulated porous structures and is evenly distributed on flexible carbon cloth fiber surface, improved on the whole as sodium-ion battery The electrochemistry cycle performance of negative electrode material.
To achieve the above object, the present invention is to be achieved through the following technical solutions:
A kind of system of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery Preparation Method, comprising the following steps:
Step 1: carbon cloth being placed in acetone to cleaning, drying after impregnating removal surface impurity, then the carbon cloth of drying is soaked into merging Coating processing is carried out in polyacrylic acid aqueous solution, cleaning is dried again；
Step 2: 0.3~1.14g antimony trichloride is added in 20~60mL dehydrated alcohol stirring, and to form antimony trichloride molten Liquid, into antimony trichloride solution, addition sodium hydrate aqueous solution adjusts its pH to 8~12 and obtains mixed liquor；By the carbon after coating processing It is arranged into mixed liquor and impregnates；
Step 3: step 2 gained carbon cloth and mixed liquor are gone into hydro-thermal reaction, cooling at 120~180 DEG C in reaction kettle Carbon cloth is taken out to room temperature, cleaning, drying obtains antimony pentoxide/polyacrylic acid/carbon cloth flexibility sodium-ion battery of reticulated porous structures Negative electrode material.
Further, soaking time is 24~72h in step 1 carbon cloth merging acetone.
Further, the mass concentration of polyacrylic acid aqueous solution is 1~8mg/mL in step 1, and the carbon cloth of drying soaks merging The time that coating processing is carried out in polyacrylic acid aqueous solution is 1~12h.
Further, polyacrylic acid average molecular weight is 1250000.
Further, it cleans in step 1 and step 3 to be cleaned repeatedly with deionized water and ethyl alcohol respectively.
Further, it is impregnated in the carbon cloth merging mixed liquor in step 2 after coating processing and stirs 20~40min.
Further, the mass concentration of sodium hydrate aqueous solution is 0.03~0.12g/mL in step 2.
Further, reaction kettle is polytetrafluoroethylkettle kettle in step 3, and carbon cloth and mixed liquor go to polytetrafluoroethylkettle kettle juxtaposition 4~48h of hydro-thermal reaction in homogeneous reaction instrument.
Further, carbon cloth is hydrophilic carbon cloth and specification is 4cm*2cm..
Compared with prior art, the following beneficial technical effect of present invention tool:
The present invention provides a kind of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility sodium-ion batteries The preparation method of negative electrode material, the preparation method are coated by the way that the carbon cloth after cleaning to be impregnated in polyacrylic acid aqueous solution Processing；Carbon cloth is then taken out to wash and dry；The carbon cloth after drying is put into antimony trichloride ethanol solution again, with sodium hydroxide Aqueous solution is precipitating reagent, then carries out hydro-thermal reaction, and antimony pentoxide/polyacrylic acid/carbon cloth that reticulated porous structures are made is soft Property anode material of lithium-ion battery；A layer polypropylene acid high polymer binder is coated in carbon cloth substrate, it not only can be with carbon cloth Substrate forms preferable combination, while polyacrylic acid intramolecular contains a large amount of carboxyl, and is evenly distributed, energy and Sb2O5Form jail Solid chemical bonding, overcome that carbon cloth surfaces are smooth, and specific surface energy is larger, load other electroactive substances can exist it is uniform The problems such as property is poor, easy to fall off；In addition, polyacrylic acid has good shape-retaining ability, satisfactory mechanical property in the electrolytic solution；Meanwhile it passing through Carbon cloth oxygen-containing functional group after crossing polyacrylic acid impregnation is abundant without being activated, and antimony pentoxide grows into unique net It the porous structure of shape and is evenly distributed on flexible carbon cloth fiber surface, which combines carbon cloth flexibility and five oxidations two The height ratio capacity of antimony improves the electrochemistry cycle performance as anode material of lithium-ion battery on the whole；Preparation method Simple and novel, short preparation period, repeatability is high, is suitble to large-scale production preparation.
Detailed description of the invention
Fig. 1 is antimony pentoxide/polyacrylic acid/carbon cloth flexibility sodium ion of reticulated porous structures prepared by embodiment 3 The X-ray diffracting spectrum of cell negative electrode material；
Fig. 2 is antimony pentoxide/polyacrylic acid/carbon cloth flexibility sodium ion of reticulated porous structures prepared by embodiment 3 The stereoscan photograph of cell negative electrode material；
Fig. 3 is antimony pentoxide/polyacrylic acid/carbon cloth flexibility sodium ion of reticulated porous structures prepared by embodiment 3 The electrochemistry cycle performance figure of cell negative electrode material.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and It is not to limit.
Embodiment 1:
A kind of system of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery Preparation Method, comprising the following steps:
Step 1: the hydrophilic carbon cloth that specification is 4cm*2cm is placed in 50mL acetone after impregnating removal surface impurity for 24 hours, It is cleaned up, will be dried at carbon cloth placement in an oven 60 DEG C repeatedly with deionized water and dehydrated alcohol respectively；Again by drying Carbon cloth, which is placed in 1mg/mL polyacrylic acid aqueous solution, keeps 1h to carry out coating processing, respectively repeatedly with deionized water and dehydrated alcohol It cleans up, will be dried again at carbon cloth placement in an oven 60 DEG C；Wherein, polyacrylic acid average molecular weight is 1250000；
Step 2: 0.3g antimony trichloride being added to magnetic agitation in 20mL dehydrated alcohol and forms antimony trichloride solution, to three The sodium hydrate aqueous solution that 0.06g/mL is added in antimony chloride solution adjusts its pH to 8 and obtains mixed liquor；By the carbon after coating processing It is arranged into mixed liquor and impregnates simultaneously magnetic agitation 30min；
Step 3: step 2 gained carbon cloth and mixed liquor being gone in polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument Hydro-thermal reaction 48h at 120 DEG C, is cooled to room temperature taking-up carbon cloth, and cleaning, drying obtains antimony pentoxide/poly- third of reticulated porous structures Olefin(e) acid/carbon cloth flexibility anode material of lithium-ion battery.
Embodiment 2:
A kind of system of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery Preparation Method, comprising the following steps:
Step 1: the hydrophilic carbon cloth that specification is 4cm*2cm is placed in 50mL acetone after impregnating 36h removal surface impurity, It is cleaned up, will be dried at carbon cloth placement in an oven 60 DEG C repeatedly with deionized water and dehydrated alcohol respectively；Again by drying Carbon cloth, which is placed in 3mg/mL polyacrylic acid aqueous solution, keeps 1h to carry out coating processing, respectively repeatedly with deionized water and dehydrated alcohol It cleans up, will be dried again at carbon cloth placement in an oven 60 DEG C；Wherein, polyacrylic acid average molecular weight is 1250000；
Step 2: 0.57g antimony trichloride is added to magnetic agitation in 20mL dehydrated alcohol and forms antimony trichloride solution, to The sodium hydrate aqueous solution that 0.08g/mL is added in antimony trichloride solution adjusts its pH to 10 and obtains mixed liquor；After coating processing Carbon cloth, which is placed in mixed liquor, impregnates simultaneously magnetic agitation 30min；
Step 3: step 2 gained carbon cloth and mixed liquor being gone in polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument Hydro-thermal reaction 48h at 150 DEG C, is cooled to room temperature taking-up carbon cloth, and cleaning, drying obtains antimony pentoxide/poly- third of reticulated porous structures Olefin(e) acid/carbon cloth flexibility anode material of lithium-ion battery.
Embodiment 3:
A kind of system of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery Preparation Method, comprising the following steps:
Step 1: the hydrophilic carbon cloth that specification is 4cm*2cm is placed in 50mL acetone after impregnating 72h removal surface impurity, It is cleaned up, will be dried at carbon cloth placement in an oven 60 DEG C repeatedly with deionized water and dehydrated alcohol respectively；Again by drying The molten middle holding 3h of aqueous solution that carbon cloth is placed in 6mg/mL polyacrylic acid carries out coating processing, uses deionized water and dehydrated alcohol respectively It cleans up, will be dried again at carbon cloth placement in an oven 60 DEG C repeatedly；Wherein, polyacrylic acid average molecular weight is 1250000；
Step 2: 0.57g antimony trichloride is added to magnetic agitation in 20mL dehydrated alcohol and forms antimony trichloride solution, to The sodium hydrate aqueous solution that 0.06g/mL is added in antimony trichloride solution adjusts its pH to 9 and obtains mixed liquor；After coating processing Carbon cloth, which is placed in mixed liquor, impregnates simultaneously magnetic agitation 30min；
Step 3: step 2 gained carbon cloth and mixed liquor being gone in polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument Hydro-thermal reaction 12h at 180 DEG C, is cooled to room temperature taking-up carbon cloth, and cleaning, drying obtains antimony pentoxide/poly- third of reticulated porous structures Olefin(e) acid/carbon cloth flexibility anode material of lithium-ion battery.
As shown in Figure 1, analyzing antimony pentoxide/polyacrylic acid/carbon with Rigaku D/max2000PCX- x ray diffractometer x The Sb that cloth flexibility anode material of lithium-ion battery, discovery sample and PDF number are 11-06902O5Structure is consistent.The sample is used The field emission scanning electron microscope of FEI Co., U.S. S-4800 type is observed, as shown in Figure 2, it can be seen that mesh structural porous Antimony pentoxide/polyacrylic acid of structure/carbon cloth flexibility anode material of lithium-ion battery.As shown in figure 3, with five prepared oxygen Change two antimony/polyacrylic acid/carbon cloth be anode material of lithium-ion battery, be assembled into CR2032 type battery, with blue electrical measurement test system into The test of row cycle performance, shows higher electrochemistry capacitance and stability.
Embodiment 4:
A kind of system of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery Preparation Method, comprising the following steps:
Step 1: the hydrophilic carbon cloth that specification is 4cm*2cm is placed in 50mL acetone after impregnating 72h removal surface impurity, It is cleaned up, will be dried at carbon cloth placement in an oven 60 DEG C repeatedly with deionized water and dehydrated alcohol respectively；Again by drying Carbon cloth, which is placed in 8mg/mL polyacrylic acid aqueous solution, keeps 1h to carry out coating processing, respectively repeatedly with deionized water and dehydrated alcohol It cleans up, will be dried again at carbon cloth placement in an oven 60 DEG C；Wherein, polyacrylic acid average molecular weight is 1250000；
Step 2: 1.14g antimony trichloride is added to magnetic agitation in 40mL dehydrated alcohol and forms antimony trichloride solution, to The sodium hydrate aqueous solution that 0.06g/mL is added in antimony trichloride solution adjusts its pH to 9 and obtains mixed liquor；After coating processing Carbon cloth, which is placed in mixed liquor, impregnates simultaneously magnetic agitation 30min；
Step 3: step 2 gained carbon cloth and mixed liquor being gone in polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument Hydro-thermal reaction for 24 hours, is cooled to room temperature taking-up carbon cloth at 180 DEG C, and cleaning, drying obtains antimony pentoxide/poly- third of reticulated porous structures Olefin(e) acid/carbon cloth flexibility anode material of lithium-ion battery.
Embodiment 5:
A kind of system of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery Preparation Method, comprising the following steps:
Step 1: the hydrophilic carbon cloth that specification is 4cm*2cm is placed in 50mL acetone after impregnating 72h removal surface impurity, It is cleaned up, will be dried at carbon cloth placement in an oven 60 DEG C repeatedly with deionized water and dehydrated alcohol respectively；Again by drying Carbon cloth, which is placed in 6mg/mL polyacrylic acid aqueous solution, keeps 2h to carry out coating processing, respectively repeatedly with deionized water and dehydrated alcohol It cleans up, will be dried again at carbon cloth placement in an oven 60 DEG C；Wherein, polyacrylic acid average molecular weight is 1250000；
Step 2: 0.57g antimony trichloride is added to magnetic agitation in 40mL dehydrated alcohol and forms antimony trichloride solution, to The sodium hydrate aqueous solution that 0.06g/mL is added in antimony trichloride solution adjusts its pH to 12 and obtains mixed liquor；After coating processing Carbon cloth, which is placed in mixed liquor, impregnates simultaneously magnetic agitation 30min；
Step 3: step 2 gained carbon cloth and mixed liquor being gone in polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument Hydro-thermal reaction 48h at 180 DEG C, is cooled to room temperature taking-up carbon cloth, and cleaning, drying obtains antimony pentoxide/poly- third of reticulated porous structures Olefin(e) acid/carbon cloth flexibility anode material of lithium-ion battery.
Embodiment 6:
A kind of system of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery Preparation Method, comprising the following steps:
Step 1: the hydrophilic carbon cloth that specification is 4cm*2cm is placed in 50mL acetone after impregnating 48h removal surface impurity, It is cleaned up, will be dried at carbon cloth placement in an oven 60 DEG C repeatedly with deionized water and dehydrated alcohol respectively；Again by drying The molten middle holding 12h of aqueous solution that carbon cloth is placed in 5mg/mL polyacrylic acid carries out coating processing, uses deionized water and anhydrous second respectively Alcohol cleans up repeatedly, will dry again at carbon cloth placement in an oven 60 DEG C；Wherein, polyacrylic acid average molecular weight is 1250000；
Step 2: 1.14g antimony trichloride is added to magnetic agitation in 60mL dehydrated alcohol and forms antimony trichloride solution, to The sodium hydrate aqueous solution that 0.03g/mL is added in antimony trichloride solution adjusts its pH to 10 and obtains mixed liquor；After coating processing Carbon cloth, which is placed in mixed liquor, impregnates simultaneously magnetic agitation 20min；
Step 3: step 2 gained carbon cloth and mixed liquor being gone in polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument Hydro-thermal reaction 4h at 180 DEG C, is cooled to room temperature taking-up carbon cloth, and cleaning, drying obtains antimony pentoxide/poly- third of reticulated porous structures Olefin(e) acid/carbon cloth flexibility anode material of lithium-ion battery.
Embodiment 7:
A kind of system of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery Preparation Method, comprising the following steps:
Step 1: the hydrophilic carbon cloth that specification is 4cm*2cm is placed in 50mL acetone after impregnating 48h removal surface impurity, It is cleaned up, will be dried at carbon cloth placement in an oven 60 DEG C repeatedly with deionized water and dehydrated alcohol respectively；Again by drying The molten middle holding 1h of aqueous solution that carbon cloth is placed in 7mg/mL polyacrylic acid carries out coating processing, uses deionized water and dehydrated alcohol respectively It cleans up, will be dried again at carbon cloth placement in an oven 60 DEG C repeatedly；Wherein, polyacrylic acid average molecular weight is 1250000；
Step 2: 0.57g antimony trichloride is added to magnetic agitation in 30mL dehydrated alcohol and forms antimony trichloride solution, to The sodium hydrate aqueous solution that 0.12g/mL is added in antimony trichloride solution adjusts its pH to 11 and obtains mixed liquor；After coating processing Carbon cloth, which is placed in mixed liquor, impregnates simultaneously magnetic agitation 40min；
Step 3: step 2 gained carbon cloth and mixed liquor being gone in polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument Hydro-thermal reaction 36h at 150 DEG C, is cooled to room temperature taking-up carbon cloth, and cleaning, drying obtains antimony pentoxide/poly- third of reticulated porous structures Olefin(e) acid/carbon cloth flexibility anode material of lithium-ion battery.
In short, the present invention carries out coating processing by the way that the carbon cloth after cleaning to be impregnated in polyacrylic acid aqueous solution；Then It takes out carbon cloth deionized water and ethyl alcohol washs repeatedly, it is spare after dry；The carbon cloth after drying is put into antimony trichloride ethyl alcohol again In solution, using sodium hydrate aqueous solution as precipitating reagent, hydro-thermal reaction is carried out, the antimony pentoxide of reticulated porous structures/poly- is made Acrylic acid/carbon cloth flexibility sodium-ion battery cathode.Operation of the present invention is simple, reproducible, after polyacrylic acid impregnation Carbon cloth oxygen-containing functional group it is abundant without being activated, antimony pentoxide grows into unique mesh structural porous structure and uniformly point For cloth on flexible carbon cloth fiber surface, which combines the height ratio capacity of carbon cloth flexibility and antimony pentoxide, from entirety On improve electrochemistry cycle performance as anode material of lithium-ion battery.
The foregoing is a further detailed description of the present application in conjunction with specific implementation manners, and it cannot be said that this Shen Specific implementation please is only limited to these instructions.For those of ordinary skill in the art to which this application belongs, it is not taking off Under the premise of from the application design, several simple deductions and replacement can also be made, all shall be regarded as belonging to the protection of the application Range.

Claims (9)

1. a kind of preparation of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery Method, which comprises the following steps:
Step 1: carbon cloth being placed in acetone to cleaning, drying after impregnating removal surface impurity, then the carbon cloth leaching of drying is placed in poly- third Coating processing is carried out in olefin(e) acid aqueous solution, cleaning is dried again；
Step 2: 0.3~1.14g antimony trichloride is added to stirring in 20~60mL dehydrated alcohol and forms antimony trichloride solution, to Addition sodium hydrate aqueous solution adjusts its pH to 8~12 and obtains mixed liquor in antimony trichloride solution；Carbon cloth after coating processing is set Enter in mixed liquor and impregnates；
Step 3: step 2 gained carbon cloth and mixed liquor being gone into reaction kettle the hydro-thermal reaction at 120~180 DEG C, are cooled to room Temperature takes out carbon cloth, and cleaning, drying obtains antimony pentoxide/polyacrylic acid/carbon cloth flexibility sodium-ion battery cathode of reticulated porous structures Material.
2. antimony pentoxide/polyacrylic acid of a kind of reticulated porous structures/carbon cloth flexibility sodium ion electricity according to claim 1 The preparation method of pond negative electrode material, which is characterized in that soaking time is 24~72h in the step 1 carbon cloth merging acetone.
3. antimony pentoxide/polyacrylic acid of a kind of reticulated porous structures/carbon cloth flexibility sodium ion electricity according to claim 1 The preparation method of pond negative electrode material, which is characterized in that the mass concentration of polyacrylic acid aqueous solution is 1~8mg/ in the step 1 ML, the carbon cloth leaching of drying, which is placed in polyacrylic acid aqueous solution, carries out the time of coating processing as 1~12h.
4. antimony pentoxide/polyacrylic acid of a kind of reticulated porous structures/carbon cloth flexibility sodium ion electricity according to claim 3 The preparation method of pond negative electrode material, which is characterized in that the polyacrylic acid average molecular weight is 1250000.
5. antimony pentoxide/polyacrylic acid of a kind of reticulated porous structures/carbon cloth flexibility sodium ion electricity according to claim 1 The preparation method of pond negative electrode material, which is characterized in that cleaning is respectively with deionized water and ethyl alcohol in the step 1 and step 3 It cleans repeatedly.
6. antimony pentoxide/polyacrylic acid of a kind of reticulated porous structures/carbon cloth flexibility sodium ion electricity according to claim 1 The preparation method of pond negative electrode material, which is characterized in that impregnated simultaneously in the carbon cloth merging mixed liquor in the step 2 after coating processing Stir 20~40min.
7. antimony pentoxide/polyacrylic acid of a kind of reticulated porous structures/carbon cloth flexibility sodium ion electricity according to claim 1 The preparation method of pond negative electrode material, which is characterized in that in the step 2 mass concentration of sodium hydrate aqueous solution be 0.03~ 0.12g/mL。
8. antimony pentoxide/polyacrylic acid of a kind of reticulated porous structures/carbon cloth flexibility sodium ion electricity according to claim 1 The preparation method of pond negative electrode material, which is characterized in that reaction kettle is polytetrafluoroethylkettle kettle, carbon cloth and mixed liquor in the step 3 It goes to polytetrafluoroethylkettle kettle and is placed in 4~48h of hydro-thermal reaction in homogeneous reaction instrument.
9. antimony pentoxide/polyacrylic acid of a kind of reticulated porous structures/carbon cloth flexibility sodium ion electricity according to claim 1 The preparation method of pond negative electrode material, which is characterized in that the carbon cloth is hydrophilic carbon cloth and specification is 4cm*2cm..
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